Usually, cold working strengthen metals and alloys by introducing large population of dislocations, whereas annealing of cold worked metal recovers the structure, annihilates dislocations, forms new strain-free grains, and results loss of strength. Here, we report annealing-hardening at temperature well below stress relieving and recrystallization temperatures in contrast to the typical behavior. A large amount of structural defects, such as dislocations, grain boundaries, twins, and stacking faults, have been introduced in nanostructured α-brass by cryorolling. The interaction and rearrangement of these defects upon annealing at 165–200 °C have been monitored at an interval of 1 minute. Large increase of the yield strength up to 578 MPa has been achieved in annealed specimens, which is 23% higher than that of as-cryorolled, and 425% higher than that of as-cast brass due to the evolution of nano-twins. Our approach shows a new avenue on strengthening fcc crystals by incorporating annealing induced nano-twins.
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